Fingerprint Construction and Identification of Common Peaks for Tenghuang Jiangu Wan Based on UPLC-Q TOF-MSE

doi:10.19894/j.issn.1000-0518.230355

Chinese Journal of Applied Chemistry ›› 2024, Vol. 41 ›› Issue (3): 437-444.DOI: 10.19894/j.issn.1000-0518.230355

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Fingerprint Construction and Identification of Common Peaks for Tenghuang Jiangu Wan Based on UPLC-Q TOF-MS^E

Dong XIE¹, Jian-Nan HU¹, Nian LI¹, Ju YANG², Qing HUANG², Zi-Feng PI¹(), Fei ZHENG¹, Yu-Lin DAI¹, Hao YUE¹()

^1.Jilin Ginseng Acadmg，Changchun University of Chinese Medicine，Changchun 130117，China
^2.Changchun People Pharmaceutical Group Co. ，Ltd. ，Changchun 130033，China

Received:2023-11-10 Accepted:2024-03-01 Published:2024-03-01 Online:2024-04-09
Contact: Zi-Feng PI,Hao YUE
Supported by:
Science and Technology Development Project of Jilin Province(20210401064YY)

1. Supporting Information.pdf(291KB)

Abstract

Abstract:

To establish the high performance liquid chromatographic （HPLC） fingerprint of Tenghuang Jiangu Wan （THJGW） and improve its quality standard，a Waters Symmetry C18 column （150 mm×2.1 mm， 3.5 μm） was used and a gradient elution with 0.1% formic acid in water （A） and 0.1% formic acid in acetonitrile （B） was performed as the mobile phase. The flow rate was 0.4 mL/min， the column temperature was 30 ℃， the injection volume was 2 μL and the detection wavelength was 260 nm. The fingerprint of THJGW was established and analyzed for its similarity by using the “Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System （2012 version）”. The identification of common peaks was characterized by ultra performance liquid chromatography-quadrupole time of flight-mass spectrometry （UPLC-Q TOF-MS^E） combining with reference standards. The relative retention times and relative peak areas of common peaks in the fingerprints of 10 batches of Tenghuang Jiangu Wan were calculated. A total of 20 common peaks were determined in the fingerprints of 10 batches from THJGW， and the similarities were all above 0.95. Based on the information of reference standards and tandem mass spectrometry， the structures of 13 components in the common peaks were identified. And then， the corresponding Chinese medicines for each peak were attributed. The relative retention times and relative peak areas of common peaks in all batches of samples were relatively stable， corresponding to a constant content of ingredients. The similarity of the intermediates was evaluated using this fingerprint and showed a good correlation between intermediates and finished products. This method is precise， reproducible and stabilized. It can be used not only for quality control of the finished product of THJGW， but also for the detection of the intermediates.

Key words: Tenghuang Jiangu Wan, High performance liquid chromatographic, Fingerprint, Ultra performance liquid chromatography-quadrupole time of flight-mass spectrometry

CLC Number:

O656

Dong XIE, Jian-Nan HU, Nian LI, Ju YANG, Qing HUANG, Zi-Feng PI, Fei ZHENG, Yu-Lin DAI, Hao YUE. Fingerprint Construction and Identification of Common Peaks for Tenghuang Jiangu Wan Based on UPLC-Q TOF-MS^E[J]. Chinese Journal of Applied Chemistry, 2024, 41(3): 437-444.

Figures/Tables 7

References 19

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Peaks （No.）	Retention time/min	Selected ion	Observed（m/z）	Mass error/（mg·L^-1）	Major product ions （m/z）	Compound	Attribution
1	4.13	［M－H］^－	331.103 8	1.0	179.056 0	Koaburaside	a
2	5.95	［M－H］^－	595.166 5	-0.7	459.113 7， 235.024 5	Neoeriocitrin	b
3	9.12	［M+H］⁺	825.278 9	-2.8	663.229 9， 517.170 4， 355.118 0	Diphylloside A	c
5	18.37	［M－H］^－	785.250 6	-0.4	623.218 8， 461.166 0， 179.034 7	Echinacoside	d
7	22.14	［M－H］^-	623.197 6	-0.9	461.164 9， 315.104 8， 179.035 5	Acteoside	d，e
8	23.61	［M－H］^－	579.171 2	-1.2	271.060 7， 151.003 3	Naringin	b
9	24.14	［M+H］⁺	273.075 9	0.6	153.018 1， 119.049 2	Naringenin	b
10	27.06	［M－H］^－	753.224 8	0.2	223.060 4， 205.050 3， 190.026 6	3，6-Disinapoyl sucrose	f
11	28.23	［M+HCOO］^－	853.276 7	-0.6	645.218 2， 366.110 4， 351.087 0	Epimedin B	c
12	34.51	［M+HCOO］^－	721.234 3	-0.8	513.175 9， 367.117 5， 351.086 6	Icariin	c
13	34.81	［M－H］^－	659.233 5	-1.6	367.116 5， 351.086 9， 323.092 0	2-O-Rhamnosylicariside Ⅱ	c
17	40.36	［M－H］^－	529.170 6	-1.8	367.117 7， 352.092 9	Icariside Ⅰ	c
19	41.39	［M－H］^－	513.176 0	-1.2	367.116 4， 352.091 2， 324.096 6	Icariside Ⅱ	c

Peaks （No.）	Retention time/min	Selected ion	Observed（m/z）	Mass error/（mg·L^-1）	Major product ions （m/z）	Compound	Attribution
1	4.13	［M－H］^－	331.103 8	1.0	179.056 0	Koaburaside	a
2	5.95	［M－H］^－	595.166 5	-0.7	459.113 7， 235.024 5	Neoeriocitrin	b
3	9.12	［M+H］⁺	825.278 9	-2.8	663.229 9， 517.170 4， 355.118 0	Diphylloside A	c
5	18.37	［M－H］^－	785.250 6	-0.4	623.218 8， 461.166 0， 179.034 7	Echinacoside	d
7	22.14	［M－H］^-	623.197 6	-0.9	461.164 9， 315.104 8， 179.035 5	Acteoside	d，e
8	23.61	［M－H］^－	579.171 2	-1.2	271.060 7， 151.003 3	Naringin	b
9	24.14	［M+H］⁺	273.075 9	0.6	153.018 1， 119.049 2	Naringenin	b
10	27.06	［M－H］^－	753.224 8	0.2	223.060 4， 205.050 3， 190.026 6	3，6-Disinapoyl sucrose	f
11	28.23	［M+HCOO］^－	853.276 7	-0.6	645.218 2， 366.110 4， 351.087 0	Epimedin B	c
12	34.51	［M+HCOO］^－	721.234 3	-0.8	513.175 9， 367.117 5， 351.086 6	Icariin	c
13	34.81	［M－H］^－	659.233 5	-1.6	367.116 5， 351.086 9， 323.092 0	2-O-Rhamnosylicariside Ⅱ	c
17	40.36	［M－H］^－	529.170 6	-1.8	367.117 7， 352.092 9	Icariside Ⅰ	c
19	41.39	［M－H］^－	513.176 0	-1.2	367.116 4， 352.091 2， 324.096 6	Icariside Ⅱ	c

Batch No.	X1	X2	X3	X4	X5	X6	X7	X8	X9	X10	R
X1	1.000	0.998	0.997	0.998	0.959	0.982	0.980	0.959	0.979	0.967	0.991
X2	0.998	1.000	1.000	0.999	0.968	0.987	0.986	0.966	0.984	0.973	0.995
X3	0.997	1.000	1.000	0.999	0.970	0.987	0.987	0.967	0.984	0.973	0.995
X4	0.998	0.999	0.999	1.000	0.964	0.984	0.983	0.962	0.980	0.969	0.992
X5	0.959	0.968	0.970	0.964	1.000	0.994	0.994	0.996	0.993	0.994	0.988
X6	0.982	0.987	0.987	0.984	0.994	1.000	0.999	0.992	0.998	0.995	0.998
X7	0.980	0.986	0.987	0.983	0.994	0.999	1.000	0.992	0.997	0.995	0.997
X8	0.959	0.966	0.967	0.962	0.996	0.992	0.992	1.000	0.996	0.998	0.987
X9	0.979	0.984	0.984	0.980	0.993	0.998	0.997	0.996	1.000	0.998	0.997
X10	0.967	0.973	0.973	0.969	0.994	0.995	0.995	0.998	0.998	1.000	0.991
R	0.991	0.995	0.995	0.992	0.988	0.998	0.997	0.987	0.997	0.991	1.000

Batch No.	X1	X2	X3	X4	X5	X6	X7	X8	X9	X10	R
X1	1.000	0.998	0.997	0.998	0.959	0.982	0.980	0.959	0.979	0.967	0.991
X2	0.998	1.000	1.000	0.999	0.968	0.987	0.986	0.966	0.984	0.973	0.995
X3	0.997	1.000	1.000	0.999	0.970	0.987	0.987	0.967	0.984	0.973	0.995
X4	0.998	0.999	0.999	1.000	0.964	0.984	0.983	0.962	0.980	0.969	0.992
X5	0.959	0.968	0.970	0.964	1.000	0.994	0.994	0.996	0.993	0.994	0.988
X6	0.982	0.987	0.987	0.984	0.994	1.000	0.999	0.992	0.998	0.995	0.998
X7	0.980	0.986	0.987	0.983	0.994	0.999	1.000	0.992	0.997	0.995	0.997
X8	0.959	0.966	0.967	0.962	0.996	0.992	0.992	1.000	0.996	0.998	0.987
X9	0.979	0.984	0.984	0.980	0.993	0.998	0.997	0.996	1.000	0.998	0.997
X10	0.967	0.973	0.973	0.969	0.994	0.995	0.995	0.998	0.998	1.000	0.991
R	0.991	0.995	0.995	0.992	0.988	0.998	0.997	0.987	0.997	0.991	1.000

Batch No.	R	Z1	Z2	Z3	Z4	Z5	Z6	Z7	Z8	Z9	Z10
R	1.000	0.975	0.981	0.985	0.981	0.995	0.998	0.998	0.995	0.998	0.997
Z1	0.975	1.000	0.995	0.997	0.997	0.956	0.981	0.974	0.954	0.980	0.968
Z2	0.981	0.995	1.000	0.999	0.999	0.967	0.988	0.983	0.961	0.984	0.971
Z3	0.985	0.997	0.999	1.000	0.999	0.972	0.990	0.986	0.967	0.987	0.976
Z4	0.981	0.997	0.999	0.999	1.000	0.965	0.987	0.981	0.961	0.984	0.972
Z5	0.995	0.956	0.967	0.972	0.965	1.000	0.993	0.994	0.995	0.990	0.991
Z6	0.998	0.981	0.988	0.990	0.987	0.993	1.000	0.997	0.991	0.997	0.993
Z7	0.998	0.974	0.983	0.986	0.981	0.994	0.997	1.000	0.991	0.995	0.993
Z8	0.995	0.954	0.961	0.967	0.961	0.995	0.991	0.991	1.000	0.994	0.997
Z9	0.998	0.980	0.984	0.987	0.984	0.990	0.997	0.995	0.994	1.000	0.998
Z10	0.997	0.968	0.971	0.976	0.972	0.991	0.993	0.993	0.997	0.998	1.000

Fingerprint Construction and Identification of Common Peaks for Tenghuang Jiangu Wan Based on UPLC-Q TOF-MS^E

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